JP2002293613A - Green, translucent alumina polycrystal body and method of producing the same - Google Patents
Green, translucent alumina polycrystal body and method of producing the sameInfo
- Publication number
- JP2002293613A JP2002293613A JP2001097715A JP2001097715A JP2002293613A JP 2002293613 A JP2002293613 A JP 2002293613A JP 2001097715 A JP2001097715 A JP 2001097715A JP 2001097715 A JP2001097715 A JP 2001097715A JP 2002293613 A JP2002293613 A JP 2002293613A
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- oxide
- weight
- sagger
- green
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6587—Influencing the atmosphere by vaporising a solid material, e.g. by using a burying of sacrificial powder
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、装飾品や宝飾品等
の工芸品、あるいは食器等の陶芸品等に利用できる透光
性アルミナ多結晶体とその製造方法に関し、特に透光性
の高いグリーン色に発色するグリーン色透光性アルミナ
多結晶体とその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a translucent alumina polycrystal which can be used for crafts such as ornaments and jewelry or ceramics such as tableware, and a method for producing the same. The present invention relates to a green translucent alumina polycrystal that develops a green color and a method for producing the same.
【０００２】[0002]
【従来の技術および発明が解決しようとする課題】従
来、装飾品や宝飾品で用いられている着色した透光性の
あるアルミナとしてはサファイアやルビー等がある。2. Description of the Related Art Conventionally, sapphire, ruby, and the like have been used as colored translucent aluminas used in ornaments and jewelry.
【０００３】アルミナはガラスに比べて硬度が非常に高
く、しかも屈折率が高いために、傷つきにくく、光沢や
輝きがガラスに比べて非常に優れており、装飾材料とし
て最適である。これらは合成宝石として、ベルヌイ法、
ＣＺ法、あるいはＦＺ法等の単結晶育成法により製造さ
れている。[0003] Alumina is very hard as compared with glass and has a high refractive index, so that it is not easily scratched, and is very excellent in gloss and shine as compared with glass, and thus is most suitable as a decorative material. These are synthetic jewels, the Bernoulli method,
It is manufactured by a single crystal growing method such as the CZ method or the FZ method.
【０００４】しかし、このプロセスでは形状や大きさに
制限があり、多大な時間と手数を要するために非常に高
価になるという問題があった。However, in this process, there is a problem that the shape and the size are limited, and a great deal of time and labor are required, so that the process becomes very expensive.
【０００５】これらの問題を解決する方法として、アル
ミナに酸化クロムと酸化マグネシウムを用いて加圧成形
した後、減圧中で焼成し、透光性の高いレッドのアルミ
ナ多結晶体を得られる方法が知られている。As a method for solving these problems, there is a method in which alumina is press-formed using chromium oxide and magnesium oxide, and then calcined under reduced pressure to obtain a red alumina polycrystal having high translucency. Are known.
【０００６】さらに近年、着色剤としての酸化コバルト
の添加量を必要最小限に抑え、焼結助剤としても有効な
着色剤である希土類を添加し、減圧下でアルミナ匣鉢に
入れて焼成することにより、鮮やかな赤味のある濃いブ
ルーを呈し、非常に透光性が高く、サファイアと比較し
ても遜色のない装飾性の高いサファイアブルーに発色す
る透光性アルミナ多結晶体を得ることができている（特
願平１2-１９４３９７号）。In recent years, the amount of cobalt oxide added as a colorant has been minimized, and rare earth, which is also a colorant effective as a sintering aid, has been added. By this, it is possible to obtain a translucent alumina polycrystal that exhibits a bright reddish dark blue, has a very high translucency, and develops a highly decorative sapphire blue that is comparable to sapphire (Japanese Patent Application No. 12-194397).
【０００７】このように透光性が高く、装飾性に優れた
アルミナ装飾材料として、レッドやブルー等の製造方法
はあるものの、カラーバリエーションとしてはまだまだ
乏しいため、装飾部材としての用途の幅が狭いものであ
った。As described above, although there are production methods of red and blue as an alumina decoration material having high translucency and excellent decoration, there are still few color variations, so the range of application as a decoration member is narrow. Was something.
【０００８】[0008]
【課題を解決するための手段】本発明は、上記事情に鑑
みて鋭意研究を重ねた結果、着色剤としての酸化ニッケ
ルの添加量を必要最小限に抑え、焼結助剤としても有効
な着色剤である希土類を添加し、減圧下でアルミナ匣鉢
に入れて予備焼成し、さらにアルミナ粉末に埋めてアル
ミナ匣鉢に入れてＨＩＰ処理し、さらに大気雰囲気で焼
成することにより、鮮やかなグリーンを呈し、非常に透
光性の高い透光性アルミナ多結晶体を得ることを知見し
た。In view of the above circumstances, the present invention has made intensive studies, and as a result, it has been found that the amount of nickel oxide added as a coloring agent is minimized and that the coloring is effective as a sintering aid. Rare earth as an agent is added, put in an alumina sagger under reduced pressure, pre-fired, buried in alumina powder, put in an alumina sagger, HIPed, and fired in the air atmosphere to produce a bright green It was found that a highly translucent alumina polycrystal having high translucency was obtained.
【０００９】本発明はこのような知見に基づいてなされ
たものであり、請求項１に係るグリーン色透光性アルミ
ナ多結晶は、アルミナ９８．５〜９９．８重量％と、酸
化ニッケル０．１〜０．５重量％とを含有するととも
に、酸化ネオジウム、酸化プラセオジム、または酸化ユ
ーロピウムのいずれか１種以上を０．１〜１．０重量％
含有してなる。The present invention has been made on the basis of such findings, and the green translucent alumina polycrystal according to claim 1 has 98.5 to 99.8% by weight of alumina and 0.1% of nickel oxide. 1 to 0.5% by weight, and 0.1 to 1.0% by weight of at least one of neodymium oxide, praseodymium oxide and europium oxide.
It contains.
【００１０】また、請求項２に係るグリーン色透光性ア
ルミナ多結晶体の製造方法では、アルミナ９８．５〜９
９．８重量％と、酸化ニッケル０．１〜０．５重量％
と、酸化ネオジウム、酸化プラセオジム、または酸化ユ
ーロピウムのいずれか１種以上が０．１〜１．０重量％
の混合物を成形し、脱脂した後、 アルミナ匣鉢に入れ
て、真空度１０Ｐａ以下の１６００℃以上で予備焼成
し、更にアルミナ匣鉢に入れて、アルミナ粉末に埋めた
後、２００ＭＰａの１５００℃以上でＨＩＰ処理し、最
後に大気雰囲気の１２００〜１６００℃で２時間以上焼
成する。According to a second aspect of the present invention, there is provided a method for producing a green translucent polycrystalline alumina.
9.8% by weight and nickel oxide 0.1 to 0.5% by weight
And at least one of neodymium oxide, praseodymium oxide, and europium oxide is 0.1 to 1.0% by weight.
After the mixture is molded and degreased, it is put in an alumina sagger, pre-fired at 1600 ° C. or more with a vacuum degree of 10 Pa or less, further put in an alumina sagger, and buried in alumina powder, and then 1500 MPa or more at 200 MPa. And finally baking at 1200 to 1600 ° C. in the air atmosphere for 2 hours or more.
【００１１】[0011]
【発明の実施の形態】以下、本発明の実施の形態を説明
する。本発明に係るグリーン色アルミナ多結晶体は、ア
ルミナ９８．５〜９９．８重量％と酸化ニッケル０．１
〜０．５重量％とを含有するとともに、酸化ネオジウ
ム、酸化プラセオジム、若しくは酸化ユーロピウムのい
ずれか１種を０．１〜１．０重量％含有してなる。Embodiments of the present invention will be described below. The green alumina polycrystal according to the present invention comprises 98.5 to 99.8% by weight of alumina and 0.1% of nickel oxide.
And 0.5% by weight, and 0.1 to 1.0% by weight of any one of neodymium oxide, praseodymium oxide and europium oxide.
【００１２】アルミナ原料は、純度９９．９％以上のも
を用い、不純物による可視光線領域の固有吸収を抑制さ
せる必要がある。It is necessary to use an alumina raw material having a purity of 99.9% or more to suppress the intrinsic absorption of impurities in the visible light region by impurities.
【００１３】酸化ニッケルはアルミナとスピネルを形成
し、酸化雰囲気焼成ではグリーン着色剤としての働きが
あるが、酸化ニッケルの添加量が０．１重量％未満で
は、緑味が弱く、 ０．５重量％を超えると焼成時の酸
化ニッケルの気化によるボイドが多発し、透光性が著し
く低下する。[0013] Nickel oxide forms a spinel with alumina and functions as a green colorant when baked in an oxidizing atmosphere. %, A large number of voids are generated due to vaporization of the nickel oxide during firing, and the light transmittance is significantly reduced.
【００１４】また、酸化ネオジウム、酸化プラセオジ
ム、若しくは酸化ユーロピウムのいずれか１種以上を添
加することで焼結助剤（粒成長抑制剤）としての働きと
ブルー系の着色剤としての働きを兼ね備え、透光性の向
上を図ると共に青味を濃くすることができる。但し、酸
化ネオジウム或いは、酸化プラセオジム若しくは酸化ユ
ーロピウムの添加量が０．１重量％未満では、発色と透
光性のいずれにも効果がなく、１．０重量％を超える
と、コランダムと光学的特性の異なるガーネットの量が
多くなるため、異相に基づく散乱が大きくなって透光性
が低下する。Further, by adding at least one of neodymium oxide, praseodymium oxide and europium oxide, it has both a function as a sintering aid (grain growth inhibitor) and a function as a blue-based coloring agent. The translucency can be improved and the bluish color can be deepened. However, if the amount of neodymium oxide or praseodymium oxide or europium oxide is less than 0.1% by weight, there is no effect on both color development and translucency. Since the amount of garnets different from each other increases, the scattering based on the different phases increases, and the light transmittance decreases.
【００１５】本発明に係る透光性アルミナ多結晶体の製
造方法は、上記組成の原料に、ポリカルボン酸アンモニ
ウム塩の分散剤、アクリル系のバインダー、ＰＥＧ系の
消泡剤、及びイオン交換水又は蒸留水を回転ボールミル
で混合してスラリーを作製する。このスラリーを攪拌真
空脱泡機で脱泡した後に、鋳込み成形し、大気雰囲気で
仮焼（６００〜１１００℃、１ｈｒ）して脱脂処理を行
った後、図１に示すように、純度９９％以上のアルミナ
匣鉢１に入れて真空度１０Ｐａ以下の１６００℃以上で
真空炉で予備焼成する。なお、アルミナ匣鉢１は、環状
のリング３の上下開口部を蓋２で覆蓋して構成され、内
部に焼成品５を配設して焼成するものである。[0015] The method for producing a translucent polycrystalline alumina according to the present invention is characterized in that a raw material having the above composition is added to a dispersant of an ammonium polycarboxylate, an acrylic binder, a PEG-based defoamer, and ion-exchanged water. Alternatively, a slurry is prepared by mixing distilled water with a rotary ball mill. After defoaming this slurry with a stirring vacuum defoaming machine, it was cast and molded, and calcined (at 600 to 1100 ° C. for 1 hour) in an air atmosphere to perform a degreasing treatment. It is placed in the above alumina sagger 1 and preliminarily fired in a vacuum furnace at 1600 ° C. or higher with a degree of vacuum of 10 Pa or lower. The alumina sagger 1 is configured by covering the upper and lower openings of an annular ring 3 with a lid 2, and has a fired product 5 disposed therein and fired.
【００１６】脱脂処理をしない場合は、減圧焼成におい
て灰分が残留して密度が上がらないため、透光性は低下
する。また、真空炉焼成でなく大気雰囲気で予備焼成す
ると焼結体内部の大きな気孔を取り除けないため、最後
に酸化焼成する際にＨＩＰで小さくした大きなボイドの
残留応力によって割れやすくなる。When the degreasing treatment is not performed, the ash remains in the calcination under reduced pressure and the density does not increase, so that the light transmittance is reduced. In addition, when pre-firing in an air atmosphere instead of firing in a vacuum furnace, large pores inside the sintered body cannot be removed, so that when oxidizing and firing at the end, cracks easily occur due to residual stress of large voids reduced by HIP.
【００１７】また、アルミナ匣鉢に入れずに焼成すると
減圧雰囲気の容積が大きくなるため、ピグメントの蒸発
が活性化すると共に、真空炉内部の炉材が全てカーボン
であるため、焼成時に焼結体が還元されて酸素欠陥が多
くなり、その結果、発色が淡く黒ずむという問題が発生
する。更に、アルミナ匣鉢の純度が、９９％未満である
と、アルミナ匣鉢の不純物が蒸発して、焼結体を汚染
し、透光性を低下させる。また、アルミナ匣鉢を用いる
ことで、他のピグメントの蒸発による汚染が著しく抑制
できるため、一度の真空炉焼成で様々な着色透光性アル
ミナを焼成できるという効果もある。Further, if sintering is not performed in an alumina sagger, the volume of the reduced-pressure atmosphere becomes large, so that the evaporation of the pigment is activated. In addition, since the furnace material inside the vacuum furnace is entirely carbon, the sintered body is not baked. Is reduced to increase the number of oxygen vacancies, and as a result, there arises a problem that the color development becomes pale and dark. Further, when the purity of the alumina sagger is less than 99%, impurities in the alumina sagger evaporate, contaminate the sintered body, and lower the light transmittance. Further, by using an alumina sagger, contamination due to evaporation of other pigments can be remarkably suppressed, so that there is an effect that various colored translucent aluminas can be fired in a single vacuum furnace firing.
【００１８】次ぎに、図２に示すように、アルミナ匣鉢
１に入れて、アルミナ粉末４に埋めた後、Ａｒ雰囲気２
００ＭＰａの１５００℃以上でＨＩＰ処理する。これに
より透光性を著しく向上させることができる。Next, as shown in FIG. 2, the sample is put in an alumina sagger 1 and buried in alumina powder 4, and then an Ar atmosphere 2
HIP processing is performed at 1500 ° C. or more of 00 MPa. Thereby, the translucency can be significantly improved.
【００１９】アルミナ粉末（敷き粉）４に埋めてＨＩＰ
処理をしなければ、真空炉焼成と同様に、焼結体が還元
されて酸素欠陥が多くなり、その結果、発色が淡く黒ず
むという問題が発生する。また、２００ＭＰａ未満、１
５００℃未満でＨＩＰ処理した場合、焼結体中のボイド
を無くすことができず、欠陥による光の散乱が減らない
ため、透光性を上げることができない。HIP embedded in alumina powder (spreading powder) 4
If the treatment is not performed, as in the case of firing in a vacuum furnace, the sintered body is reduced and the number of oxygen vacancies increases, and as a result, there occurs a problem that the color development becomes pale and dark. In addition, less than 200 MPa, 1
When the HIP treatment is performed at a temperature lower than 500 ° C., voids in the sintered body cannot be eliminated and light scattering due to defects does not decrease, so that the light transmittance cannot be increased.
【００２０】最後に、大気雰囲気の１２００〜１６００
℃で２時間以上焼成することで、トルコブルー色の焼結
体をグリーンにすることができる。Finally, the atmosphere of 1200 to 1600
By firing at 2 ° C. for 2 hours or more, the Turkish blue sintered body can be made green.
【００２１】１２００℃未満で焼成した場合は、部分的
にトルコブルーの発色が残って完全なグリーンになら
ず、また１６００℃以上で焼成すると、ＨＩＰ処理で小
さくしたボイドが元に戻り、その結果、磁器の割れや透
光性の低下につながる。When fired at a temperature lower than 1200 ° C., the color of Turkish blue partially remains and the green color is not obtained. When fired at a temperature of 1600 ° C. or more, the voids reduced by the HIP treatment return to the original state. This can lead to cracking of the porcelain and a decrease in light transmission.
【００２２】[0022]
【実施例】アルミナ（Ａｌ2Ｏ3）に酸化ニッケル（Ｎｉ
Ｏ）、酸化ネオジウム（Ｎｄ2Ｏ3）、酸化プラセオジム
（Ｐｒ5Ｏ11）、または酸化ユーロピウム（Ｅｕ2Ｏ3）
を各々所定量添加し、更にイオン交換水、分散剤として
ポリカルボン酸アンモニウム塩、バインダーとしてのポ
リアクリル酸、及び消泡剤としてポリエチレングリコー
ルを加え、ボールミルで１６時間混合した。これらのス
ラリーを２５μｍの篩に通し、３０分間攪拌真空脱泡し
た。さらにこのスラリーを加圧鋳込み成形し、脱脂のた
めに大気中の９００℃で１時間保持して仮焼した。EXAMPLE Alumina (Al 2 O 3 ) has nickel oxide (Ni
O), neodymium oxide (Nd 2 O 3 ), praseodymium oxide (Pr 5 O 11 ), or europium oxide (Eu 2 O 3 )
Were added in predetermined amounts, and ion-exchanged water, ammonium polycarboxylate as a dispersant, polyacrylic acid as a binder, and polyethylene glycol as an antifoaming agent were further added, and mixed with a ball mill for 16 hours. These slurries were passed through a 25 μm sieve, and the mixture was degassed under vacuum for 30 minutes. The slurry was cast under pressure, and calcined at 900 ° C. in the atmosphere for one hour for degreasing.
【００２３】その後、一部は真空炉で０．１Ｐａの１７
００℃で３時間保持し、一部は大気雰囲気の１７００℃
で時間保持し、図１に示すように、純度９９％のアルミ
ナ匣鉢に入れて予備焼成した。Thereafter, a part of the pressure was 0.1 Pa 17 in a vacuum furnace.
Hold at 00 ° C for 3 hours, partly at 1700 ° C in air
, And as shown in FIG. 1, it was placed in an alumina sagger of 99% purity and preliminarily fired.
【００２４】さらに、図２に示すように、アルミナ匣鉢
に入れて、一部アルミナ粉末に埋めた後、Ａｒ雰囲気の
２００ＭＰａ、所定温度で１時間保持してＨＩＰ処理し
た。Further, as shown in FIG. 2, the sample was placed in an alumina sagger, partially filled with alumina powder, and then subjected to HIP treatment at 200 MPa in an Ar atmosphere at a predetermined temperature for 1 hour.
【００２５】最後に、大気雰囲気の所定温度で２時間焼
成し、グリーン磁器を作製した。Finally, it was fired at a predetermined temperature in the air atmosphere for 2 hours to produce a green porcelain.
【００２６】これら焼結体を厚さ２ｍｍに研削し、鏡面
研磨後、発色は目視により評価し、透光性は、分光測色
計（ミノルタ製ＣＭ−３７００ｄ）を用い、基準光源Ｄ
６５で、波長範囲３６０〜７４０ｎｍの光透過率を測定
し、平均光透過率を求めた。これらの結果を表１に示
す。These sintered bodies were ground to a thickness of 2 mm, and after mirror polishing, the color development was visually evaluated. The translucency was measured using a spectrocolorimeter (CM-3700d manufactured by Minolta).
At 65, the light transmittance in the wavelength range of 360 to 740 nm was measured, and the average light transmittance was determined. Table 1 shows the results.
【００２７】なお、予備焼成欄では、真空炉焼成したも
のは“Ｖ”、大気雰囲気で焼成したものは“Ｏ”と表示
した。埋め焼き欄ではＨＩＰ処理時に埋め処理したもの
は“○”、していないものは“×”と表示した。さら
に、透光性の評価については平均光透過率が１０％以上
のものは“○”、１０％未満のものは“×”と表示し、
クラックについては発生したものは“×”、発生しなか
ったものは“○”と表示した。In the column of pre-firing, "V" was obtained for firing in a vacuum furnace, and "O" was obtained for firing in an air atmosphere. In the fill-in field, those that have been filled during HIP processing are indicated by ““ ”, and those that have not been filled are indicated by“ x ”. Further, regarding the evaluation of the translucency, those having an average light transmittance of 10% or more are indicated by "O", and those having an average light transmittance of less than 10% are indicated by "X",
Regarding cracks, those that occurred were indicated by “x”, and those that did not occur were indicated by ““ ”.
【００２８】[0028]
【表１】 [Table 1]
【００２９】表１から明らかなように、予備焼成を大気
雰囲気で行うと透光性が低下し、クラックが発生する。
また、ＨＩＰ処理温度が１５００℃未満では透光性が低
く、ＨＩＰ処理時に埋め焼きをしないと発色が暗くなっ
た。さらに、最後の発色調整のための焼成温度は、１２
００℃未満では部分的にトルコブルー色が残り、完全な
グリーン色にならなかった。As is evident from Table 1, when the pre-firing is performed in the air atmosphere, the light transmittance decreases and cracks occur.
Further, when the HIP processing temperature was lower than 1500 ° C., the light transmittance was low, and the color was darkened without burying and burning during the HIP processing. Further, the firing temperature for the final color adjustment is 12
If the temperature is lower than 00 ° C., a part of Turkish blue color remains, and a complete green color is not obtained.
【００３０】そして、組成においては、酸化ニッケルの
添加量が０．１重量％未満では、緑味が弱く、 ０．５
重量％を超えると透光性が著しく低下した。In the composition, when the amount of nickel oxide added is less than 0.1% by weight, the greenness is weak, and
When the content is more than the weight%, the light transmittance is remarkably reduced.
【００３１】また、酸化ネオジウム、酸化プラセオジ
ム、若しくは酸化ユーロピウムのいずれか１種以上を添
加することで透光性が向上すると共に青味を濃くするこ
とができた。但し、酸化ネオジウム、酸化プラセオジ
ム、若しくは酸化ユーロピウムの添加量が０．１重量％
未満では、発色と透光性のいずれにも効果がなく、１．
０重量％を超えると、透光性が低下した。Further, by adding at least one of neodymium oxide, praseodymium oxide and europium oxide, the translucency was improved and the bluish color could be deepened. However, the addition amount of neodymium oxide, praseodymium oxide, or europium oxide is 0.1% by weight.
If it is less than 1, there is no effect on both coloring and translucency.
If it exceeds 0% by weight, the light transmittance is reduced.
【００３２】[0032]
【発明の効果】以上のように、請求項１に係る透光性ア
ルミナによれば、アルミナ９８．５〜９９．８重量％、
酸化ニッケル０．１〜０．５重量％、酸化ネオジウム、
酸化プラセオジム、又は酸化ユーロピウムのいずれか１
種が０．１〜１．０重量％からなることから、従来にな
いエメラルドの透明感と深みのある装飾性の高いグリー
ン素材が簡単で安価に作れ、しかも形状や大きさに制限
されることなく、エメラルドグリーンに発色する透光性
アルミナ製品を作ることができる。As described above, according to the translucent alumina according to claim 1, 98.5 to 99.8% by weight of alumina,
0.1 to 0.5% by weight of nickel oxide, neodymium oxide,
Either praseodymium oxide or europium oxide
Since the seeds consist of 0.1 to 1.0% by weight, an emerald transparent material with a high degree of decorativeness that is unprecedented can be easily and inexpensively made, and is limited in shape and size. In addition, a translucent alumina product that develops emerald green can be produced.
【００３３】また、請求項２に係る透光性アルミナの製
造方法によれば、アルミナ９８．５〜９９．８重量％、
酸化ニッケル０．１〜０．５重量％、酸化ネオジウム或
いは酸化プラセオジ若しくは酸化ユーロピウムを０．１
〜１．０重量％の混合物を成形し、脱脂した後、 アル
ミナ匣鉢に入れて、真空度１０Ｐａ以下の１６００℃以
上で予備焼成し、更にアルミナ匣鉢に入れて、アルミナ
粉末に埋めた後、２００ＭＰａで１５００℃以上でＨＩ
Ｐ処理し、最後に大気雰囲気にて１２００〜１６００℃
で２時間以上焼成することにより、従来にないエメラル
ドの透明感と深みのある装飾性の高いグリーン素材が簡
単で安価に作れ、しかも形状や大きさに制限されること
なく、エメラルドグリーンに発色する透光性アルミナ製
品を作ることができる。Further, according to the method for producing translucent alumina according to claim 2, 98.5 to 99.8% by weight of alumina,
0.1 to 0.5% by weight of nickel oxide, 0.1% by weight of neodymium oxide or praseodymium or europium oxide
After molding and degreased a mixture of about 1.0% by weight, the mixture was placed in an alumina sagger, pre-baked at 1600 ° C. or higher with a vacuum degree of 10 Pa or less, further placed in an alumina sagger, and embedded in alumina powder. HI at 1500 MPa or more at 200 MPa
P treatment, and finally 1200 to 1600 ° C in air atmosphere
Baking for more than 2 hours makes it possible to easily and inexpensively create an emerald transparent and deep decorative high-definition green material without any restrictions on shape and size, and develops into emerald green Translucent alumina products can be made.
【図１】本発明の製造方法で用いられる真空焼成用アル
ミナ匣鉢を示す図である。FIG. 1 is a view showing an alumina sagger for vacuum firing used in a production method of the present invention.
【図２】本発明の製造方法で用いられるＨＩＰ処理用ア
ルミナ匣鉢を示す図である。FIG. 2 is a view showing an alumina sagger for HIP processing used in the production method of the present invention.
１：アルミナ匣鉢、４：アルミナ粉末、５：焼成品 1: alumina sagger, 4: alumina powder, 5: fired product
Claims (2)
酸化ニッケル０．１〜０．５重量％とを含有するととも
に、酸化ネオジウム、酸化プラセオジム、または酸化ユ
ーロピウムのいずれか１種以上を０．１〜１．０重量％
含有してなるグリーン色透光性アルミナ多結晶体。1. An alumina having a content of 98.5 to 99.8% by weight,
0.1 to 0.5% by weight of nickel oxide, and 0.1 to 1.0% by weight of at least one of neodymium oxide, praseodymium oxide and europium oxide
A green translucent alumina polycrystal containing.
酸化ニッケル０．１〜０．５重量％と、酸化ネオジウ
ム、酸化プラセオジム、または酸化ユーロピウムのいず
れか１種以上が０．１〜１．０重量％の混合物を成形
し、脱脂した後、アルミナ匣鉢に入れて、真空度１０Ｐ
ａ以下の１６００℃以上で予備焼成し、更にアルミナ匣
鉢に入れて、アルミナ粉末に埋めた後、２００ＭＰａの
１５００℃以上でＨＩＰ処理し、最後に大気雰囲気の１
２００〜１６００℃で２時間以上焼成するグリーン色透
光性アルミナ多結晶体の製造方法。2. 98.5 to 99.8% by weight of alumina;
A mixture of 0.1 to 0.5% by weight of nickel oxide and 0.1 to 1.0% by weight of at least one of neodymium oxide, praseodymium oxide, and europium oxide is formed, degreased, and then alumina box. Put in a pot, vacuum 10P
a, pre-fired at 1600 ° C. or higher, further placed in an alumina sagger, buried in alumina powder, HIPed at 1500 ° C. or higher at 200 MPa, and finally
A method for producing a green translucent alumina polycrystal which is fired at 200 to 1600 ° C. for 2 hours or more.
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|---|---|---|---|
| JP2001097715A JP2002293613A (en) | 2001-03-29 | 2001-03-29 | Green, translucent alumina polycrystal body and method of producing the same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001097715A JP2002293613A (en) | 2001-03-29 | 2001-03-29 | Green, translucent alumina polycrystal body and method of producing the same |
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| Publication Number | Publication Date |
|---|---|
| JP2002293613A true JP2002293613A (en) | 2002-10-09 |
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ID=18951459
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|---|---|---|---|
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| JP2011524846A (en) * | 2008-06-19 | 2011-09-08 | ダウ グローバル テクノロジーズ エルエルシー | Additives containing cellulose ether for ceramic extrusion |
| JP2013523573A (en) * | 2010-04-01 | 2013-06-17 | ロレックス・ソシエテ・アノニム | Alumina-based opaque ceramics |
| CN117264440A (en) * | 2023-11-14 | 2023-12-22 | 山东陶正新材料科技有限公司 | Manufacturing process of black pigment for high-temperature-resistant alumina and zirconia ceramics |
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| JP2011524846A (en) * | 2008-06-19 | 2011-09-08 | ダウ グローバル テクノロジーズ エルエルシー | Additives containing cellulose ether for ceramic extrusion |
| WO2010058745A1 (en) | 2008-11-18 | 2010-05-27 | 東ソー株式会社 | Sintered colored alumina of high toughness and high translucency, and manufacturing method and uses therefor |
| US8481439B2 (en) | 2008-11-18 | 2013-07-09 | Tosoh Corporation | Colored alumina sintered body of high toughness and high translucency, and its production method and its uses |
| EP2808313A2 (en) | 2008-11-18 | 2014-12-03 | Tosoh Corporation | Colored alumina sintered body of high toughness and high translucency, and its production method and its uses |
| JP2013523573A (en) * | 2010-04-01 | 2013-06-17 | ロレックス・ソシエテ・アノニム | Alumina-based opaque ceramics |
| CN117264440A (en) * | 2023-11-14 | 2023-12-22 | 山东陶正新材料科技有限公司 | Manufacturing process of black pigment for high-temperature-resistant alumina and zirconia ceramics |
| CN117264440B (en) * | 2023-11-14 | 2024-01-30 | 山东陶正新材料科技有限公司 | Manufacturing process of black pigment for high-temperature-resistant alumina and zirconia ceramics |
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